AEROSPACE AMS2643 REV.

E
MATERIAL
Issued 1972-11
SPECIFICATION Revised 2012-09

Superseding AMS2643D
Structural Examination of Titanium Alloys
Chemical Etch Inspection Procedure

RATIONALE

This document revision removes the requirement for heat treatment of macrostructure specimens to avoid conflict with
OEM procedures and clarifies inspection procedure.

1. SCOPE

1.1 Purpose

This specification covers a procedure for revealing the macrostructure and microstructure of titanium alloys.

1.2 Application

This inspection procedure has been used typically for detecting defects and segregation in titanium alloys. This procedure
should not be used on finished parts.

1.3 Safety - Hazardous Materials

While the materials, methods, applications, and processes described or referenced in this specification may involve the
use of hazardous materials, this specification does not address the hazards which may be involved in such use. It is the
responsibility of the user to ensure familiarity with the safe and proper use of any hazardous materials and to take
necessary precautionary measures to ensure the health and safety of all personnel involved.

2. APPLICABLE DOCUMENTS

The issue of the following document in effect on the date of the purchase order forms a part of this specification to the
extent specified herein. The supplier may work to a subsequent revision of a document unless a specific document issue
is specified. When the referenced document has been canceled and no superseding document has been specified, the
last published issue of that document shall apply.

2.1 ASME Publications

Available from American Society of Mechanical Engineers, 22 Law Drive, P.O. Box 2900, Fairfield, NJ 07007-2900,
Tel: 973-882-1170, www.asme.org.

ASME B 46.1 Surface Texture, Roughness, Waviness and Lay

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Copyright © 2012 SAE International
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3. TECHNICAL REQUIREMENTS

3.1 Materials and Solutions

3.1.1 Specimens for Revealing Macrostructure

3.1.1.1 Bars, Extrusions, Plates, and Stock for Forging or Extruding

Specimens shall be transverse cross-sections not less than 0.50 inch (12.7 mm) thick cut from the product to be tested in
the transverse direction. Surface roughness shall be of 70 microinches (1.8 µm) AA or less, determined in accordance with
ASME B 46.1.

3.1.1.2 Forgings

When dimensions permit, forgings shall be rough-machined to clean up and to ensure freedom from alpha case. A
minimum of 0.030 inch (0.76 mm) of material shall be left on the surfaces of the forgings between final etching and finish
machined configuration to ensure freedom from intergranular attack and hydrogen pickup on finished parts. If forgings are
to be inspected by ultrasonic inspection procedures, the configuration used for such inspection is acceptable. Surface
roughness shall be 130 microinches (3.3 µm) AA or less, determined in accordance with ASME B 46.1.

3.1.2 Specimens for Revealing Microstructure

The specimens on which macrostructure was revealed shall be sectioned through any areas of concern and, also, where
practical, shall be sectioned for examination of other planes as needed to provide representative sampling of the product.

3.2 Equipment

3.2.1 The etchant tank, fixtures, racks, and baskets shall be lined/coated with or fabricated from a material that will not
react with the etchant (See Table 1).

3.2.2 The tank shall be equipped with exhaust ventilation to vent gases from the vigorous reaction.

3.3 Preparation

Specimens shall be free from water breaks. If water breaks are observed, parts shall be recleaned and reinspected for
water break until no water breaks are observed.

3.4 Procedure

3.4.1 Macrostructure Inspection

3.4.1.1 Macrostructure etch

Specimens shall be etched in an aqueous acid solution, maintained at room temperature, for sufficient time to develop a
well-defined macrostructure (See 8.2). The solution in Table 1, or an alternative solution acceptable to purchaser, shall be
used.

TABLE 1 - ETCHANT

Ingredient Grams per liter

Nitric Acid, Technical Grade 142 ± 20
Hydrofluoric Acid, Technical Grade 60 ± 9
Water Balance
* Expressed as HNO3 or HF respectively by mass.

The etching rate of the solution shall be maintained to remove 0.002 to 0.004 inch (0.05 to 0.10 mm) of metal in a five
minute period.
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3.4.1.2 Rinse and Dry

Specimens shall be rinsed immediately in clean water for several minutes followed, as required, by pressurized spraying or
wiping with a cloth to remove smut.

Remove water from specimens by blowing dry with clean air.

3.4.1.3 Inspection

Specimens shall be visually inspected for macrostructure and indications of defects, such as segregation, (See 8.2), laps,
folds, cracks, and inclusions, using 1X magnification and a light intensity not lower than 200 foot-candles (2153 lx).

3.4.1.3.1 Specimens showing significant indications shall be evaluated as necessary to interpret the indications, by
additional sectioning and repeated macroscopic etch and inspection, or microstructure inspection (3.4.2), as
needed.

3.4.2 Microstructure Inspection

If examination of the macrostructure indicates the need for further evaluation, the microstructure shall be developed as
follows:

3.4.2.1 The specimens to be examined shall be polished and etched using metallographic techniques that will clearly
reveal the microstructure to be evaluated (See 8.3).

3.4.2.2 The specimens shall be examined to determine the microstructure and the nature of indications found in the
macrostructure.

4. QUALITY ASSURANCE PROVISIONS

4.1 Acceptance Tests

Tests for macrostructure (3.4.1) and, when applicable, microstructure (3.4.2) shall be performed to determine product
acceptance.

4.2 Periodic Test

The test to maintain the etchant solution (3.4.1.1) is a periodic test and shall be performed at a frequency selected by the
processor unless frequency of testing is specified by the cognizant engineering organization. See 8.4.

5. PREPARATION FOR DELIVERY

Not applicable.

6. ACKNOWLEDGMENT

The processor shall mention this specification number and its revision letter in all quotations and when acknowledging
purchase orders.

7. REJECTIONS

Not applicable.

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8. NOTES

8.1 A change bar (l) located in the left margin is for the convenience of the user in locating areas where technical
revisions, not editorial changes, have been made to the previous issue of this specification. An (R) symbol to the left
of the document title indicates a complete revision of the specification, including technical revisions. Change bars
and (R) are not used in original publications, nor in specifications that contain editorial changes only.

8.2 Segregation

Segregation is similar to other material defects in that it can occur throughout the product in any frequency, size, shape,
form, or severity. However, the extreme ends of the ingot are most likely to have segregation.Segregation will appear, after
macroetching, as an area of high silvery luster on a matte grey background. Typical segregation in titanium 6Al-4V alloy
billet is shown in Figure 1. Segregation can be distinguished from staining or other discoloration by rubbing the surface
with a rubber eraser. Segregation cannot be rubbed out whereas staining or discoloration will disappear. After segregation
has been obliterated by rubbing with abrasive paper, it will reappear after localized re-etching.

8.3 The preferred procedure for preparing specimens for examination of microstructure is as follows:

8.3.1 Polish electrolytically in the following solution at 40 volts ± 1 direct current for approximately five seconds:
78 mL perchloric acid
120 mL reagent water (See ASTM D 1193 Type II)
700 mL ethanol
100 mL 2-butoxy ethanol

8.3.2 Etch with Kroll's reagent (5% hydrofluoric acid, (sp gr 1.15), 12% nitric acid, (sp gr 1.42), 83% water, by volume),
for sufficient time to develop the microstructure, wash in warm running water, and dry. Specimens may be rinsed
in a solution of sodium bicarbonate and again rinsed in warm running water, if desired, between the rinsing and
drying operations.

8.3.3 Mechanical polishing or other suitable means may be used provided equivalent microstructural presentations are
developed.

8.4 ARP4992, Periodic Test Plan for Process Solutions, is recommended to satisfy the requirements for the control of
processing solutions.

8.5 Terms used in this AMS are clarified in ARP1917.

8.6 Dimensions and properties in inch/pound units and the Fahrenheit temperatures are primary; dimensions and
properties in SI units and the Celsius temperatures are shown as the approximate equivalents of the primary units
and are presented only for information.

PREPARED BY AMS COMMITTEE “B”

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FIGURE 1 - TYPICAL SEGREGATION IN TITANIUM 6AL-4V AFTER ETCHING, 2X MAGNIFICATION

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